SG185123A1 - Nano-wires made of novel precursors and method for the production thereof - Google Patents

Nano-wires made of novel precursors and method for the production thereof Download PDF

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SG185123A1
SG185123A1 SG2012081030A SG2012081030A SG185123A1 SG 185123 A1 SG185123 A1 SG 185123A1 SG 2012081030 A SG2012081030 A SG 2012081030A SG 2012081030 A SG2012081030 A SG 2012081030A SG 185123 A1 SG185123 A1 SG 185123A1
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precursors
nanowires
nanowires according
hydrogen
deposition
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SG2012081030A
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Norbert Auner
Christian Bauch
Rumen Deltschew
Sven Holl
Gerd Lippold
Javad Mohsseni
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Spawnt Private Sarl
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Priority claimed from DE201010019565 external-priority patent/DE102010019565A1/en
Priority claimed from DE201010019874 external-priority patent/DE102010019874A1/en
Application filed by Spawnt Private Sarl filed Critical Spawnt Private Sarl
Publication of SG185123A1 publication Critical patent/SG185123A1/en

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Abstract

AbstractThe invention relates to nano-wires which consist of or comprise semiconductor materials and are used forapplications in photovoltaics and electronics and to a method for the production thereof. The nano-wires are characterized in that they are obtained by a novel method using novel precursors. The precursors represent compounds, or mixtures of compounds, each having atleast one direct Si-Si and/or Ge-Si and/or Ge-Ge bond, the substituents of which consist of halogen and/or hydrogen, and in the composition of which the atomic ratio of substituent:metalloid atoms is at least 1:1.

Description

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Description
Nano-wires made of novel precursors and method for the production thereof ’ i . } : The present invention relates to nanowires which consist of or comprise semiconductor materials and which serve for applications in photovoltaics and electronics, and also to a method for production thereof. BA feature of the nanowires 1s that they are obtained by an innovative method using innovative precursors. The precursors constitute compounds or mixtures of compounds each having at least one direct
Si-Si and/o» Ge-Si and/or Ge-Ge bond, with substituents which consist of halogen and/or hydrogen and with a composition in which the atomic ratic of substituents to metallioid atoms is at least 1:1. ’
Prior art:
Described in the prior art, for the production of silicon nanowires, is the thermal decomposition of gaseous silicon precursor compounds. Here, besides various silicon compounds, catalytically active metals are employed. Generally speaking, catalyst metal agglomerates of a few nanometers in diameter are } produced first of all, and then act catalytically on the decomposition of the silicon compounds and contribute to the ordered deposition of the elemental silicon formed. Depending on the reaction conditions, the resulting nanowires are crystalline or wholly or partly amorphous. It 1s preferred to use metals which exhibit eutectic mixtures with a low melting temperature with silicon. The model conception says 3E that, under the reaction conditions, a liquid metal/Si mixture 1s formed, from which, finally, solid Si .depcsits as a result of further uptake of Si from the
NUIT
. <
7 a . . - 2 - precursor compounds as they decompose. However, a comparable growth behavior is also observed even at temperatures below the eutectic melting point. Silicon nanowires are deposited predominantly on substrates such as silicon or such as metal oxides, an example being Al,0s5. )
For example, E.C. Garnett, W. Liang, and P. Yang,
Advanced Materials 2007, 79, 2946, describe the production of silicon nanowires by CVD deposition from
SiCl,/H», with Pt as catalyst metal, under atmospheric pressure and at 805°C. Y. Zhang, ©. Zhang, N. Wang,
Y. Yan, H. Zhou, and J. Zhu, Journal of Crystal Growth 2006, 221, 183, use a similar method under atmospheric pressure with an optimized temperature of 800°C, with : Ni as catalyst metal.
It is found that for the epitaxial deposition of silicon nanowires on crystalline silicon it is necessary first of 2ll to remove the oxide layer of the substrate. . Where chlorosilanes are used as precursor compounds, there is formation, together with hydrogen additionally present, of HCl, which reacts with the oxide layer (S. Ge, K. Jiang, X. Lu, Y. Chen, R. Wang, and S. Fan, Advanced Materials 2005, 17, 56). When chlorine-free precursor silanes are used, the same effect can be achieved by admixing HCl (S. Sharma,
T.T. Kamins, and R.S. Williams, Journal of Crystal
Growth 2004, 261, 613). For example, WO 2001/136412, after the production of suitable catalyst metal agglomerates, ciaims the successive use of at least two different precursor gas mixtures, of which the. first mixture comprises either a chlorine-containing silane or, 1n addition to a silane, another chlorine source, and which ensures the start of growth, but requires comparatively high temperatures for the decomposition.
Thereafter the reaction temperature is lowered and a r <. - 3 - second precursor gas 1s used, which has a lower decomposition temperature. Suitable precursor compounds . cited are SiHg, Si,He, SiCl;, and SiH:Cl,. Examples of suitable catalyst metals are Au, Ai, Pt, Fe, Ti, Ga,
Ni, Sn, or In. In addition to the conventional CVD technique for producing silicon nanowires, there are also references to Plasma Enhanced Sputter Deposition and Plasma Enhanced CVD, which allow a reduction in the reaction temperature. 16
W.I. Park, G. Zheng, X- Jiang, B. Tian, and
C.M. Lieber, Nano Letters 2008, 8, 3004, describe how at 400°C and 10 torr pressure, the growth rate of silicon nanowires with Au as catalyst is 130 times greater for disilane, Si;He, than for SiH.,. Even with reaction temperatures optimized for SiH4, the growth rate lags behind that starting from disilane by a factor of 31. S. Akhtar, A. Tanaka, K. Usami,
Y. Tsuchiya, and S$. Oda, Thin Solid Films 2008, 517, 317, show that nanowires can be produced from Si;Hs/H; using Au catalyst even at a temperature of 350°C and under a pressure of 3 Torr. For example,
JP 2006117475 A and JP 2007055840 2A describe the production ‘of Si nanowires at temperatures as low as 250-300°C, using disilane and trisilane as silicon sources, employing the metals Au, Ag, Fe, and/or Ni as catalysts, and setting a pressure during the reaction of 1-5 torr.
E.-Y. Tuan, D.C. Lee, T. Hanrath, and B.A. Korgel, Nano
Letters 2005, 5, 681, show that the formation of Si nanowires takes place even without a substrate in supercritical organic solvents at 400-520°C and =z pressure of 14.3 - 23.4 MPa. The catalyst metal used is
Ni, and, in addition to trisilane, Si3Hg, the precursor compounds employed include octylsilane and phenylsilane. A.T. Heitsch, D.D. Fanfeir, H.-Y. Tuan,.
' i
Co. and B.A. Korgel, Journal of the American Chemical
Society 2008, 130, 5436, show that for trisilane as precursor molecule, this reaction leads To SS. nanowires even under atmospheric pressure and at boiling temperature (420-430°C) with high-boiling organic solvents.
A disadvantage of the use of silanes (SigHon+z) 1s their pyrophoric properties (self-ignitability in air), which hinder handling. . Objective:
The object on which the present invention is based is that of providing innovative nanowires by a new method from suitable precursors of the specified kind that are new for this purpese. The intention, moreover, 1s To provide a method for producing such nanowires. 2C Definitions:
Precursors for the growth of nanowires are silicon and/or germanium-containing compounds which are converted into elemental silicon and/or germanium under the process conditions.
Polysilanes in the sense of the invention are compounds having at least one Si-Si bond. According to one embodiment of the invention, polysilanes are halogenated and hydrogenated polysilanes and ‘also polysilanes having organic supstituents, and the corresponding partially halogenated and partially hydrogenated polysilanes, having the following general : : formula: SiyX.H,, where a+b 1s greater than or equal to 2n and less than or egual to 2r+2, a and kb are each greater than or equal to 0, and X = halogen, amine substituent or organic radical, such as alkyl radicals,
’ ‘ - 5 - for example, more particularly methyl. It is also possible, furthermore, to use polysilanes with organic substituents for SiC nanowires, or with amine substituents for SiN nanowires. It 1s also possible, furthermore, <tTo0 use polysilanes having (transition) metal substituents.
Polygermanes in the sense of the invention are compounds having at least one Ge-Ge bond. According to one embodiment of the invention, the polygermanes are halogenated and hydrogenated polygermanes and also the ' corresponding partially halogenated and partially hydrogenated polygermanes, having the following general formula: GepX.H,, where a+b 1s greater than or equal to 2n and less than or equa. to 2nt+2, & and b each being greater than or equal to 0, and X = halogen, amine substituent or organic radicai, such as alkyl radicals, for example, more particularly methyl. Furthermcre, polyogermanes with organic substituents can also be used for GeC nanowires, or, with amine substituents for GeN nanowires. Tt is also possible, furthermore, for polygermanes having {transition} metal substituents to be used.
Polygermasilanes in the sense of the invention are compounds having at least one Si-Ge bond. According to one embodiment of .the invention, -poliygermas:lanes are halogenated and hydrogenated polygermasilanes, and also the corresponding partially halogenated and partially hydrogenated polygermasilanes, having the following general formula: Si,-.Ge.X.Hg or Si,Ge..X:Hy, where a+b is greater than or equal to 2n and less than or equal to 2n+Z, a and b each being greater than or egual to C, n is greater than z, and X = halogen, amine substituent or organic radical, such as alikyi radicals, for example, more particularly methyi. Additionally it 1s also possible to use polygermasilanes having organic
-¢ — substituents for $1GeC nanowires, or having amine substituents for SiGeN nanowires. Additionally it is also possible to use - polygermasilanes having (transition) metal substituents. . | : | :
By p-doped precursors 1s meant that the respective . compound/the mixture comprises a fraction of p-doping atoms such as boron, aluminum, galiium, or indium, preferably boron atoms, that is useful for the desired semiconductor properties of the deposition product (e.g., Fermi level), it being possible for these atoms either to be incorporated into the precursor molecules or to be admixed as separate compounds to the " precursors.
By n-doped precursors is meant that the respective compound/the mixture comprises a fraction of n-doping atoms such as nitrogen, phosphorus, arsenic, antimony, or bismuth, preferably phosphorus atoms, that is useful for the desired semiconductor properties of the deposition product {e.qg., Fermi level), it being possible for these atoms either to be incorporated Into the precursor molecules or to be admixed as separate compounds to the precursors. : Further doping elements may be taken from the groups of the Periodic Table of the Elements to the leit and right of main group 4 (group 14), preferably from groups 13 and 13.
Monosilanes and monogermanes are all compounds having in each case only one silicon atom or one germanium atom. SiX,H, and GeX.Hp, where a+b is 4, and a and b are each greater than or equal to O. :
The term “metalloid atoms” refers to atoms of the semimetals silicon and germanium.
+ i . : : _ : The expressions “..consist of halogen..” or “.consist of hydrogen...” mean that apart from minor other constituents (< 1% by mass), the substituents consist exclusively of halogen or of hydrogen, respectively.
By “predominantly” is meant that the constituent in ' question is present in the mixture to an extent of more than 80% by mass. oo “Virtually nolne]” means that a secondary constituent is present at less than 5% by mass in a mixture.
Description:
I) : The nanowires produced in accordance with the invention are notable for the fact that the innovative precursors used are liquid under standard conditions (room temperature, atmospheric pressure) with one exception (Si,He) and are soluble in numerous solvents, meaning that they can be handled more easily and securely than many conventional precursors, such as monosilane, for example. Examples of solvents which are inert relative to the precursors are monochlorosilanes, such as SiCly, *iquid alkanes, such as hexane, heptane, pentane, and octane, and also aromatics, such as benzene, toluene, and xylene, for example.
In certain embodiments of the invention, particularly preferred precursors are the highly chlorinated polysilanes, polygermanes, polygermasilanes, more particularly SinHalons: with Hal = Cl, ¥, Br, or I, preference being given to using ‘SipClsp.z with n= 2 -10G, more preferably with n = 2 -5. Polygermanes which can be used are, generally, compounds of the general formula GepHalonez, with. Hal = C1, F, Br, or I, preferably GepCln:s. Polygermasilanes which car be used
+ . - 8 - ’ are compounds of the general formula Sip-.GesHalsno Or
SiyGep-yHalsns, with n > x, it being possible for the parameter n in the case of the polygermanes and polygermasilanes to be n= 2 -190, more preferably n=2 -5.
According to a further embodiment of the invention, the nanowires may be obtained from precursors which contain virtually no rings, the amount of rings, based on the overall product mixture, being below < 2% by mass.
According to a further embodiment of the invention, the nanowires may be obtained from precursors which contain virtually no branched chains, the amount of branching sites, based on the overall product mixture, being below < 5% by mass, preferably < 2% by mass. It is possible, for example, to use halogenated polysilanes having a low fraction of rings and having chains with low degrees of branching, these polysilanes being of +the kind described in PCT application W02009/143823 AZ, hereby incorporated in full by reference in relation to their properties and synthesis.
Furthermore, the nanowires may be obtained Irom precursors which consist predominantly c¢f JDbranched chains. It is possible, for example, to use halogenated polysilanes having a high fraction of rings and having branched chains, of the kind described in PCT application WO 2009/143824 Al, hereby incorporated in full by reference in relation to their properties and synthesis.
According to another embodiment of the invention it is possible to obtain nanowires from precursors whose substituents consist exclusively of hydrogen. In this case, for example, polysilanes, polygermanes or pclvgermasilanes of the general formulae SinEzp-2,
Co . GepHons» and/or Sip-xGeyHonsz Or SinGen-yHynez With n > x with n = 3 -1C, more preferably with n = 3 -5, can be used as precursors. It is also possible to use cyclic polysilanes, polygermanes and polygermasilanes having the general formulae SisHzn, GepHzn and/or Si, ;GeyHazn or
SiyxGep-xHon, with n > x with n = 3 -10, more preferably with n = 4-6.
The gas mixture (precursor and carrier gas and/or hydrogen) used in the context of the method of the invention may additionally be diluted with an inert gas, such as helium, neon, argon, krypton, xenon, Or : nitrogen, for example, and/or may comprise further admixtures (additives), such as doping additives, examples being liguid or solid boron compounds, metallic compounds or phosphorus compounds, for example. Examples are BBri, TiCls, or bPCl,, In the context of the method of the invention, the admixing of : inert gases is, however, not mandatory.
The deposition temperatures in the method of the invention lie between 250 - 1100°C, preferably between 330 to 950°C.
Some embodiments of the method of the invention are notable for the fact that nanowires can be obtained from the precursors of the invention without the presence of hydrogen in free or bonded form being necessary during the deposition, since there are other semiconductor-yielding reactions present, as for example: Si3Clg => 2 SiCig + Si, GezCle -> 2 GeCl, + Ge, 3 GeSi,Cle -> 4 SiClgq + 2 GeCl, + GeSi,. In the case of certain embodiments of the invention, this is possible through use of highly halogenated, more particularly highly chlorinated, polysilanes of the general formula
SinClapsz With n = 2 -1C, more preferably with n = 2 -5, or by using the corresponding highly halogenated, more particularly high chlorinated, polygermanes or polygermasilanes. :
The reaction pressures in the case of the method of the invention are situated in the range from 0.1 hPa to 2200 hPa, preferably at 1 hPa TO 1100 hPa, more preferably between 200 hPa and 1100 hPa.
The partial pressures of the precursors of the invention may be adjusted in a simple way by varying the temperatures of the reservoir vessel and also by admixing further gas components.
Metallic catalysts employed for the deposition of the nanowires of the invention include metals such as bismuth, preferably transition metals, such as Cu, Ag,
Ni, and Pt, for example, or else Au, or mixtures thereof. }
By using the precursors of .the invention it is possible to employ catalysts which do not affect the electronic properties of the nanowires. Ni and Pt particularly are compatible with typical metal oxide semiconductor technologies. ’ According to a further embodiment of the invention, the innovative precursors are able to be decomposed over the metallic catalysts to form the corresponding elements, as for example Si or Ge, and/or alloys, as for example Si-Ge alloys, and so Zorm the nanowires.
The particle sizes (diameters) oI the catalysts are 5 nr to 1000 nm, preferably 20 nm - 200 nm, and can be determined by means of an electron microscope, for 32 axample.
The nanowires of the invention possess diameters in the range from 50 to 1200 nm and lengths in the range from 100 to 100 000 nm, and other dimensions are obtainable as well by varying the growth times. - The growth rates are situated in the range from 5 nm to 5000 nm per minute. .
By using the precursors of the invention and/or at low process temperatures of below 600°C during the formation of the nanowires, the growth of the nanowires of the invention «can also be carried out without formation of hydrogen halide, thereby exerting .an influence also on the etching behavior and the epitaxiaily associated orientation of the nanowires. ~ The precursors of the invention are preferably suitable both for the gas/liquid/solid phase growth process and for the gas/solid/solid phase growth process. In the ) case of the gas/liquid/solid phase growth process, a liquid eutectic mixture is formed from the metal and the semimetal element (e.g., gold/silicon), from which silicon deposits on the solid wire and in which fresh silicon dissolves by decomposition of the precursors in : the gas phase. In the case of the gas/solid/solid phase growth process, a solid alloy of the semimetal element in the metal is formed by the dissolution of the element after decomposition of the precursor and also by the depositior Zrom the sclid alloy onto the nanowire as a result of diffusion processes in the sclid alloy.
In the case of certain embodiments of the invention, by using the precursors of the invention, such as the highly halogenated polysilanes, polygermanes or . 35 polygermasilanes, for example, it is pessible to obtain hydrogen-Zree nanowires, since the use of hydrogen is not necessary for producing the nanowires.
AL further feature of the nanowires produced in accordance with the invention is that the innovative precursors used may be designed preferably as single- source precursors for doped semiconductor regions. As a result of this it is possible to do away with the use of toxic or otherwise hazardous dopants, such as phosphine and diborane, for example, which in conventional doping processes necessitate the use of costly gas supply and safety systems. According to one embodiment of the invention, therefore, it is possible to produce the nanowires using exclusively the precursors, without additional reactive gases, such as hydrogen, for example. 1%
Moreover, a2 feature of the nanowires produced in : accordance with the invention is that the innovative precursors used can be used in temporal alternation, i.e., for example, p-doped and n-doped precursors alternately, for the growth, with the precursors being switched at least once during the process. In this way it is pcssibie to obtain, for example, differently doped regions preferably in alternation in the longitudinal direction, more particularly p/n junctions, which are important, for example, for the photovoltaic effect. In a corresponding way it 1s also possible, furthermore, to produce alternating regions having different Si:Ge ratios.
In addition it is possible to obtain nanowires having compositions which alternate in growth direction. For this purpose, different precursors/precursor mixtures can be provided in alternation during growth. As a result it is possible to obtain, for example, different dopings or alloys in a crystal of a nanowire.
A further feature of the method of the invention for
- 13 =- producing nanowires is that during the deposition of the nanowires, besides the nanowires, less than 10% of : pulverulent by-products, comprising, for example, the elemental semimetals Si or Ge, are deposited in the deposition region of the nanowires. These unwanted by- : products may" be formed as a result of unwanted, uncatalyzed decomposition of the precursors.
All of the precursors of the invention can also be used for the epitaxial growth of nanowires on crystalline Si substrates.
Working example:
Using highly chlorinated polysilanes of the formula
SinClznsz with n = 2 -10, such as SisCls, for example, as precursors, and with Au as metallic catalyst, nanowires can be produced with decomposition of the precursors at temperatures between 400°C to 900°C. Besides the precursors, only helium, as inert gas, was present, and " so the nanowires were produced in particular in the absence of hydrogen or other reactive gases. The nanowires had dimensions of 2 um to 20 um in length, "and a width of 50 nm to 500 nm.

Claims (22)

Claims
1. Nanowires which consist of or comprise semiconductor materials and serve for applications in photovoltaics and electronics, characterized in that they are produced from precursors which constitute compounds or mixtures of compounds each having at least one direct S$i-Si and/or Ge-Si Co and/or Ge-Ge bond, with substituents consisting of halogen and/or hydrogen and with a composition in which the atomic ratio of substituents to metalloid atoms is at least 1:1.
2. The nanowires according to claim 1, characterized in that they are obtained from precursors which for deposition do not require the presence of hydrogen in free or bonded form.
3. The nanowires according to either of the preceding claims, characterized in that they are obtained } from precursors which contain virtuaily no rings, the amount of rings, based on the overall product mixture, being below < 2% by mass.
4. The nanowlres according to any of the preceding claims, characterized in that they are obtained from precursors which contain virtually no branched chains, the amount of branching sites, based on the overall product mixture, being below
<.5% by mass, preferably < 2% by mass.
5. The nanowires according to any of claims 1 to 23, characterized in that they are obtained from precursors which consist predominantly of branched chains.
6. The nanowires according to anv of the preceding claims, characterized in that they are obtained from precursors whose substituents consist exclusively 0% halogen, more’ particularly chlorine.
7. The nanowires according to any of claims 1 to 3, characterized in that they are obtained from precursors whose substituents consist exclusively of hydrogen. Co
8. The nanowires according to any of claims 1 to 4 or . 6, 7, characterized in that they are obtained from precursors which consist predominantly of linear chains.
9. The nanowires according to any of the preceding claims, characterized in that they are obtained : from precursors which possess an average chain length of n = 2-6, preferably n = 2-5.
10. The nanowires according to any of the preceding claims, characterized in that they are obtained from precursors which are readily solubie in inert solvents.
11. The nanowires according to any of the preceding claims, characterized in that they are obtained from precursors which are not pyrophoric, such as, for example, highly halogenated polysilanes, the halogen being more particularly Cl and/or Br.
12. The nanowires according to any of the preceding claims, characterized in that they contain less than 1 atom% of hydrogen. 33
13. The nanowires according to any of the preceding claims, characterized in that they contain 10 ppb to 50 000 ppm, preferably 10.ppb to 100 ppm, of halogen, preferably chlorine.
14. The nanowires according to any of the preceding claims, characterized in that they are obtained from precursors which have an H content of less than 5 atom%, preferably less than 2 atom%.
15. The nanowires according to any of the preceding claims, characterized in that they are obtained - from precursors which comprise p-doping atoms incorporated in the precursor molecules.
le. The nanowires according to any of the preceding claims, characterized in that they are obtained from precursors which comprise n-doping atoms incorporated in the precursor molecules.
17. The nanowires according to any of the preceding claims, characterized in that they are obtained from precursors which comprise p-doping additions as separate additives in the mixture.
18. The nanowires according to any of the preceding ‘claims, characterized in that they are obtained from precursors which comprise n-doping additions as separate additives in the mixture. }
12. The nanowires according to any of the preceding claims, characterized in that they are obtained from precursors which comprise doping additions from the groups of the Periodic Table of =the Elements to the left and right of main group 4 (group 14), preferably from groups 13 and 15. oo
20. The nanowires according to any of the preceding claims, characterized in thet they are obtained
3 | = 17 = from the precursors, with admixtures from the group of the monosilanes and/or the monogermanes having been added additionally.
21. The nanowires according to any of the preceding : claims, characterized in that they are obtained from precursors which are decomposed over catalysts for the deposition of the nanowires of the invention, ~ with catalysts employed being metals, preferably transition metals, or mixtures thereof.
22. The nanowires according to any of the preceding claims, characterized in that they are obtained from precursors which are suitable both for the gas/liquid/solid phase growth process and for the gas/solid/solid phase growth process.
23. A method for producing nanowires according to any of the preceding claims by reacting precursors, Or precursors and hydrogen, characterized in that a precursor:hydrogen mixing ratio of 21:0 to 1:2 000 000 is operated.
24. The method according to preceding claim 23, characterized in that the deposition takes place without presence of hydrogen in elemental or bonded form. 0
25. The method according to any of the preceding claims, characterized in that less than 10% of pulverulent by-products occur in the deposition of the nanowires.
26. The method according to any of the preceding claims, characterized in that & pressure range of
0.1 - 2200 hPa, preferably 1 to 1200 hPa is
"operated.
"27. The method according to “any of the preceding : claims, characterized in that the deposition takes place at a temperature of 250°C to 1100°C, preferably 300°C to 950°C, more preferably, "in particular 350°C to 900°C.
28. A method for producing nanowires according to any of the preceding claims by reacting precursors, or : precursors and hydrogen, characterized in that different precursors for the growth are used in : temporal alternation, the precursors being switched at least once during the process.
22. A method for producing nanowires according to any of the preceding claims by reacting precursors, or : precursors and hydrogen, characterized ir that nanowires having compositions which a_ternate in growth direction are obtained.
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